2-fluoroethanimidamide hydrochloride synthesis
- Product Name:2-fluoroethanimidamide hydrochloride
- CAS Number:2805-16-5
- Molecular formula:C2H6ClFN2
- Molecular Weight:112.5338
503-20-8
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Yield:2805-16-5 75%
Reaction Conditions:
with hydrogenchloride in ethanol at -50 - 20;
Steps:
78.A Example 78 Fluoroacetamidine
HCl gas was bubbled into fluoroacetonitrile (11 g, 186 mmol) at 0-20° C. until the reaction mixture solidified.. Precooled EtOH (40 ML) was added to solid at -50° C. and the reaction was allowed to warm to room temperature overnight.. ether (200 ML) was added and the solid product i was filtered and washed with ether to give a total of 15.72 g of white solid (yield=75%).. sodium hydroxide (4.0 g, 100 mmol) was added to a mixture of amidine i (5.63 g, 50 mmol) and ester ii (11.1 ML, 55 mmol) in EtOH (250 ML).. The suspension was heated at reflux for 7 hr.. After cooling to room temperature, the mixture was poured into water and acidified with a 10% HCl solution.. Extraction with EtOAc followed by evaporation and trituration with ether gave pyrimidone iii as a solid (2.59 g, 26% yield)..
References:
US6346534,2002,B1 Location in patent:Page column 41-42
3862-78-0
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2805-16-5
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